DE10159388A1 - Process for the production of coated bleach activator granules - Google Patents

Abstract

The aim of the invention is to improve the stability in storage and pourability of particle-shaped bleach activators of formula (I) in which: R<1> represents -H, -CH3, a C2-24 alkyl radical or alkenyl radical, a substituted C2-24 alkyl radical or alkenyl radical having at least one substituent selected from the group comprised of -Cl, -Br, -OH, -NH2, -CN, an alkyl radical or alkenyl aryl radical having a C1-24 alkyl group or represents a substituted alkyl radical or alkenyl aryl radical having a C1-24 alkyl group and at least one additional substituent on the aromatic ring; R<2> and R<3>, selected independent of one another, consist of -CH2-CN, -CH3, -CH2-CH3, -CH2-CH<2>-CH3, -CH(CH3)-CH3, -CH2-OH, -CH2-CH2-OH, -CH(OH)-CH3, -CH2-CH2-CH2-OH, -CH2-CH(OH)-CH3, -CH(OH)-CH2-CH3, -(CH2CH2-0)nH with n being equal to 1, 2, 3, 4, 5 or 6; R<4> and R<5>, independent of one another, have a meaning previously given for R<1>, R<2> or R<3>, and; X is a charge-compensating anion. The stability in storage and pourability are improved, essentially by spraying the particle-shaped bleach activators with an acid aqueous solution that, as both a coating and hardening active substance, contains polymeric polycarboxylate and/or phosphonic acid or alkali phosphonate while simultaneously drying them in a fluidized bed apparatus.

Description

The invention relates to a method for coating granules containing bleach activator by treatment with an acidic aqueous strengthening solution, which as a coating and Solidification agent contains polymeric polycarboxylate and / or alkali phosphonate, at simultaneous drying in a fluidized bed apparatus.

In addition to the ingredients that are indispensable for the washing process, such as surfactants and builder materials, detergents and cleaning agents generally contain other ingredients, which can be summarized under the term washing aids and which include such different active ingredient groups as foam regulators, graying inhibitors, bleaching agents and color transfer inhibitors. Such auxiliaries also include substances which support the surfactant performance through the oxidative degradation of soiling on the textile or such in the fleet. The same applies analogously to cleaning agents for hard surfaces. Inorganic peroxygen compounds, in particular hydrogen peroxide and solid peroxygen compounds which dissolve in water with the liberation of hydrogen peroxide, such as sodium perborate and sodium carbonate perhydrate, have long been used as oxidizing agents for disinfection and bleaching purposes. The oxidizing effect of these substances in dilute solutions depends strongly on the temperature; For example, with H ₂ O ₂ or sodium perborate in alkaline bleaching liquors, sufficiently quick bleaching of soiled textiles can only be achieved at temperatures above about 60 ° C. At lower temperatures, the oxidation effect of the inorganic peroxygen compounds can be improved by the addition of so-called bleach activators, for which numerous suggestions, especially from the substance classes of the N- or O-acyl compounds, for example multiply acylated alkylenediamines, in particular tetraacetylethylenediamine, acylated glycolurils, in particular tetraacetylglycoluril, N- acylated hydantoins, hydrazides, triazoles, Hydrotriazine, urazoles, diketopiperazines, sulfuryl amides and cyanurates, also carboxylic anhydrides, especially phthalic anhydride, Carbonsäureester, especially sodium nonanoyloxybenzenesulfonate, sodium isononanoyloxybenzenesulfonate and acylated sugar derivatives, such as pentaacetylglucose, are known in the literature. By adding these substances, the bleaching effect of aqueous peroxide liquors can be increased to such an extent that even at temperatures below 60 ° C essentially the same effects occur as with the peroxide liquor alone at 95 ° C. European patent application EP 0 464 880 discloses bleach-intensifying cationic nitriles of the general formula R'R "R""N ⁺ -CR ₁ R ₂ -CN X, in which R ₁ and R _{2 are} hydrogen or a substituent with at least one C. Atom, R 'is a C _1-24 alkyl, alkenyl or alkyl ether group or a group -CR ₁ R ₂ -CN, and R "and R"' are each a C _1-24 alkyl or hydroxyalkyl group and the counter anion X ^{- is} an organic sulfonate, an organic sulfate or a carboxylate.

From international patent application WO 98/23719 it is known that compounds of the general formula R ¹ R ² R ³ N ⁺ CH ₂ CN X ^- in which R ¹ , R ² and R ³ independently of one another have an alkyl, alkenyl or aryl group 1 to 18 carbon atoms, where the groups R ² and R ^{3 can} also be part of a heterocycle including the N atom and optionally further hetero atoms, and X is a charge-balancing anion, as activators for in particular inorganic peroxygen compounds in aqueous cleaning solutions for dishes can be used. This results in an improvement in the oxidation and bleaching effect, in particular of inorganic peroxygen compounds, at low temperatures below 80 ° C., in particular in the temperature range from approximately 15 ° C. to 55 ° C. However, the cationic nitriles, in particular in combination with other ingredients of detergents and cleaning agents, are usually not very stable in storage and are particularly sensitive to moisture.

From international patent application WO 00/50556, the manufacture is firmer Preparations containing cationic nitrile and solid carrier material by a Vacuum steam drying process known in a mixer.

The object of the invention was to provide a method which allows Granules containing a cationic nitrile, so in particulate washing and Incorporate cleaning agents that the cationic nitrile if possible, even after storage Loss of bleach activating effect. It has now been found that the Production of preparations that meet this requirement by means of a fluidized bed Wrapping process is possible. In this way, a Apply a protective coating to the granules without accepting them Bleach activator effect must be accepted.

The invention relates to a preparation of a coated particulate preparation containing a compound of the formula (I),


in which R ^{1 is} -H, -CH ₃ , a C _2-24 alkyl or alkenyl radical, a substituted C _2-24 alkyl or alkenyl radical with at least one substituent from the group -Cl, -Br, - OH, -NH ₂ , -CN, an alkyl or alkenylaryl radical with a C _1-24 alkyl group, or for a substituted alkyl or alkenylaryl radical with a C _1-24 alkyl group and at least one further substituent on the aromatic ring, R ² and R ^{3 are} independently selected from -CH ₂ -CN, -CH ₃ , -CH ₂ -CH ₃ , -CH ₂ -CH ₂ -CH ₃ , -CH (CH ₃ ) -CH ₃ , -CH ₂ - OH, -CH ₂ -CH ₂ -OH, -CH (OH) -CH ₃ , -CH ₂ -CH ₂ -CH ₂ -OH, -CH ₂ -CH (OH) -CH ₃ , -CH (OH) - CH ₂ -CH ₃ , - (CH ₂ CH ₂ -O) _n H with n = 1, 2, 3, 4, 5 or 6, R ⁴ and R ⁵ independently of one another for R ¹ , R ² or R ³ have the meaning indicated and X is a charge-balancing anion, characterized in that the bleach activator according to formula (I), which is present in solid, in particular powdery form, is desired if necessary in a mixture with binder and / or solid filler or as prefabricated granules, with simultaneous drying in a fluidized bed apparatus, sprayed with an acidic aqueous strengthening solution which contains polymeric polycarboxylate and / or phosphonic acid or alkali metal phosphonate as coating and strengthening active substance.

This makes it possible to use the bleach activator according to formula (I) completely enclose contained particles with a coating material. Moreover is when using the polymeric polycarboxylate and / or phosphonic acid or solution containing alkali phosphonate an increase in grain strength of the bleach activator particle observed.

The preparation of compounds according to formula I can by known methods or based on this, as they are for example in the patent literature or by Abraham in Progr. Phys. Org. Chem. 11 (1974), pp. 1ff, or by Arnett in J. Am. Chem. Soc. 102 (1980), p. 5892ff. have been published.

Preference is given to the use of compounds of the formula I in which R ¹ , R ² and R ^{3 are} identical. Among these, preference is given to those compounds in which the radicals mentioned mean methyl groups. On the other hand, preference is also given to those compounds in which at least 1 or 2 of the radicals mentioned are methyl groups and the others have more than one carbon atom.

The anions X ^- include in particular the halides such as chloride, fluoride, iodide and bromide, nitrate, hydroxide, phosphate, hydrogen phosphate, dihydrogen phosphate, pyrophosphate, metaphosphate, hexafluorophosphate, carbonate, hydrogen carbonate, sulfate, hydrogen sulfate, C _1-20 alkyl sulfate, C. _1-20 alkyl sulfonate, optionally C _1-18 alkyl substituted aryl sulfonate, chlorate, perchlorate and / or the anions of C _1-24 carboxylic acids such as formate, acetate, laurate, benzoate or citrate, alone or in any mixtures.

Compounds according to formula 1 are preferred in which X ^- chloride, sulfate, hydrogen sulfate, ethosulfate, C _12/18 -, C _12/16 - or C _13/15 -alkyl sulfate, lauryl sulfate, dodecylbenzenesulfonate, toluenesulfonate, cumene sulfonate, xylene sulfonate or methosulfate or Mixtures of these is. Toluene sulfonate or cumene sulfonate is understood to mean the anion of the ortho-, meta- or para-isomer of methylbenzenesulfonic acid or isopropylbenzenesulfonic acid and any mixtures thereof. Para-isopropylbenzenesulfonic acid is particularly preferred.

The compound according to general formula I can be used in solid form as such or in particulate form, that is to say applied to an organic and / or inorganic carrier material, as the starting material in the coating process according to the invention. The compound of the formula (I) can be applied to the support material in such a way that the support material is stirred into a solution of the compound of the formula I, as is obtained in the course of its preparation, and the aqueous solvent, if appropriate, in vacuo, if desired at elevated Temperature, subtracts. However, the solution of the compound of the formula I can also be sprayed onto the support material and, if appropriate, or subsequently, subjected to a drying process. Enveloping the bleach activator granules produced in accordance with the methods disclosed in German patent applications DE 197 40 668 or DE 197 40 671 is also possible by means of the method according to the invention and represents a preferred embodiment of the method according to the invention. It is preferred if the particles produced by the packaging process have a diameter in the range of 0.4 mm to 3 mm. Suitable carrier materials are all substances which do not interact in an unacceptably negative manner with the compound according to formula 1, for example alkali metal sulfonate, surfactants, organic acids and polymers, alkali metal carbonates, alkali metal sulfates, alkali metal hydrogen sulfates, alkali metal hydrogen carbonates, alkali metal phosphates, alkali metal hydrogen phosphate and alkali metal phosphate and dialkali metal alkali metal salts mixtures. Support materials are preferably used whose inner surface is in the range from 10 m ² / g to 500 m ² / g, in particular 100 m ² / g to 450 m ² / g. The silicate carrier materials which are particularly suitable in the context of the present invention include, for example, both alkali silicates and also silicas, silica gels and clays and mixtures thereof. However, the carrier material is preferably free of zeolites. In addition to the silicate component, silicate-containing carrier material optionally contains further particulate inert constituents which do not unreasonably impair the stability of the compounds of the formula I. Silicas which have been produced by a thermal process (flame hydrolysis of SiCl ₄ ) (so-called pyrogenic silicas) can be used as well as silicas produced by wet processes. Silica gels are colloidal silicas with elastic to firm consistency and a largely loose pore structure, which results in a high fluid absorption capacity. They can be produced by the action of mineral acids on water glass. Clays are naturally occurring crystalline or amorphous silicates of aluminum, iron, magnesium, calcium, potassium and sodium, for example kaolin, talc, pyrophyllite, attapulgite, sepiolite, montmorillionite and bauxite. The use of aluminum silicate as a carrier material or as a component of a carrier material mixture is also possible. The carrier material preferably has particle sizes in the range from 100 μm to 1.5 mm.

• a) Ansatz einer wäßrigen Lösung, enthaltend kationisches Nitril, vorzugsweise in Mengen von 10 Gew.-% bis 90 Gew.-%, insbesondere von 15 Gew.-% bis 50 Gew.-%, und gegebenenfalls Alkalicumolsulfonat, insbesondere Natriumcumolsulfonat,
• b) gegebenenfalls Einstellen der Lösung auf einen sauren pH-Wert, insbesondere durch Zugabe von Schwefelsäure und/oder Zitronensäure
• c) Verdüsung und Trocknung der Lösung in einer Wirbelschichtapparatur,
• d) gegebenenfalls Abpuderung des so erhaltenen Primärgranulats unter Einsatz von Kieselsäure, Zeolith und/oder Na-Cumolsulfonat in der Wirbelschicht,

durchführt und das so erhaltene gegebenenfalls abgepuderte Granulat mit der wäßrigen Verfestiger- und Umhüllungslösung bei gleichzeitiger Trocknung in der gleichen oder gegebenenfalls einer nachgeschalteten zweiten Wirbelschichtapparatur besprüht. Danach kann das Granulat aus der Wirbelschichtapparatur ausgetragen und gegebenenfalls in Gutkorn und Grob-/Feinkorn, insbesondere durch Sieben, getrennt werden. Gegebenenfalls kann sich die Rückführung von Feinkorn und/oder aufgemahlenem Grobkorn in die Wirbelschicht in Schritt c) und/oder die Rückführung von Feinkorn und/oder aufgemahlenem Grobkorn in den Abpuderungsschritt d) anschließen. In a further preferred embodiment of the invention, the steps are first carried out

• a) preparation of an aqueous solution containing cationic nitrile, preferably in amounts from 10% by weight to 90% by weight, in particular from 15% by weight to 50% by weight, and if appropriate alkali metal sulphonate, in particular sodium cumene sulphonate,
• b) if necessary, adjusting the solution to an acidic pH, in particular by adding sulfuric acid and / or citric acid
• c) atomization and drying of the solution in a fluidized bed apparatus,
• d) optionally powdering the primary granules thus obtained using silica, zeolite and / or sodium cumene sulfonate in the fluidized bed,

is carried out and the optionally powdered granules thus obtained are sprayed with the aqueous strengthening and coating solution while drying in the same or, if appropriate, a downstream second fluidized bed apparatus. The granules can then be discharged from the fluidized bed apparatus and, if necessary, separated into good and coarse / fine particles, in particular by sieving. If appropriate, the return of fine grain and / or ground coarse grain to the fluidized bed in step c) and / or the return of fine grain and / or ground coarse grain to the powdering step d) can follow.

The coated bleach activator granules obtainable by the process according to the invention or the proportion of good grain in it is preferably medium Particle diameter in the range from 0.2 mm to 2.5 mm, in particular in the range from 0.4 mm to 2.0 mm. Its bulk density is preferably in the range from 300 g / l to 1000 g / l, in particular in the range from 400 g / l to 800 g / l. The proportion of connection according to formula (I) is preferably in the range from 10% by weight to 90% by weight, in particular from 15% by weight to 50% by weight. It is preferably used for manufacturing Particulate detergent or cleaning agent used.

Fluid bed devices that can be used in a method according to the invention are for example from the European patent EP 0 603 207 B1 or the German Patent application DE 197 50 424 known. To improve the prevention of diarrhea Granules through the through openings located in the inflow floor, whereby they in Can come into contact with surfaces of relatively high temperature Openings of a grid, in particular with mesh sizes smaller than 600 μm, be covered. The grid can be inside or above the passage openings be arranged. Preferably, however, the grid is immediately below that Through openings of the inflow floor, as in principle from the German Patent application DE 197 50 424 is known. In a practical embodiment can on the underside of a known inflow floor, a metal gauze with the appropriate sintered mesh size or attached in some other way. The Metal gauze preferably consists of the same material as the inflow floor, especially made of stainless steel. With the fine-meshed grid, a failure of Particles, especially when the system stops unscheduled, but also especially in the case of particularly heavy particles with bulk densities around 1000 g / l prevented during operation. The mesh size of the above is preferably Grid network between 200 and 400 µm. It is also an advantage if the one used Inflow floor a pressure loss of at most 10 mbar and in particular at most Has 6 mbar.

According to the aqueous strengthening and coating solution in one Fluid bed apparatus applied. Coming as a hardening and coating agent polymeric polycarboxylates, in particular polymerization products of acrylic acid, Methacrylic acid or maleic acid, or copolymers of at least two of these, in question, in completely or partially neutralized form, in particular in the form of Alkali salts can be used. Alternatively or in addition to polymeric Polycarboxylate can use phosphonic acid or alkali phosphonate come. In the alkali metal salts mentioned, sodium is the preferred alkali metal in each case. It is preferred to adjust the solution to the lowest possible viscosity for good Droplet distribution during spraying into the fluidized bed with simultaneous drying. If the pH value of the solution is not in the acid range from the start, by adding acids compatible with the system, in particular by adding sulfuric acid and / or citric acid, to acidic values, in particular to values in the pH range from 4 to 4.4, set. It is preferred that - based on the granules to be coated - as much spraying the aqueous solution that the coating 1% by weight to 25% by weight, constitutes in particular 2% by weight to 15% by weight.

The granules can then be removed from the fluidized bed in a manner known in principle discharged and, if necessary, classified according to the particle size, as above executed undesirably small particles (fine grain) and undesirably large particles (Coarse grain) after a grinding step, optionally in a granulation process can be returned. In a special embodiment of the invention The classified good grain can be introduced again into a fluidized bed apparatus and sprayed on it solidifying and coating solution to make up the If necessary, to further improve the product properties of the granulate.

Granules encased by the process according to the invention are stable on storage, good free-flowing and of sufficient grain stability to be shared with others Particulate constituents of detergents or cleaning agents are mixed together can. Coated granules obtainable by the process according to the invention are in particular particulate washing or cleaning agents, preferably in such Amounts used that these agents contents from 0.1 wt .-% to 10 wt .-%, in particular from 0.2% by weight to 7% by weight of bleach activator according to formula (I).

Examples example 1

In a fluidized bed apparatus (Glatt® AGT 400 with 40 cm diameter) at 400 m ³ / h supply air flow, a supply air temperature of 95 ° C and an exhaust air temperature of 55 ° C from a homogeneous aqueous solution of trimethylammonium acetonitrile methosulfate and Na-cumolsulfonate (mass ratio 1: 1, dry matter content 30%) with a throughput of the solution of 3 kg / h within 5 h, a granulate which was still very sticky. The stickiness could be eliminated by repeated granulation with a 20% aqueous solution of polymeric polycarboxylate (Sokalan® CP45, manufacturer BASF) under the same conditions with regard to the supply air flow, supply air temperature and exhaust air temperature. The polymer content in the granules thus obtained was 5% by weight. The grain size of the granules was in the range from 0.4 mm to 2.0 mm, the bulk density was 700 g / l. The granules were then sieved and the fraction with particle sizes of between 0.8 and 1.6 mm was mixed with the other detergent components of a detergent formulation. The finished detergent could be used without clumping.

Example 2

In a fluidized bed apparatus with a diameter of 1.8 m (Glatt® AGT 1800), primary granules were produced from a 40% strength aqueous solution of the cationic nitrile used in Example 1 while being powdered with Na-cumene sulfonate powder. The supply air volume was 21000 m ³ / h, the supply air temperature was 145 ° C. The exhaust air temperature was set to 65 ° C by water evaporation of the solution. After 1 h the fluidized bed operated in batch was so full that the granulation was ended. The solidification was carried out with the 20% polymer solution used in Example 1 at a supply air of 110 ° C. The polymer content in the finished granulate was 10% by weight. The granules obtained were sieved between 0.8 and 1.6 mm. The bulk weight was 730 g / l.

The finished granulate was mixed with the usual particulate detergent components prepared a particulate detergent.

Example 3

In a fluidized bed apparatus with a diameter of 1.8 m (Glatt® AGT 1800), primary granules were produced from a 40% strength aqueous solution of the cationic nitrile used in Example 1, with powdering with silica powder (Tixosil® 38A). The supply air volume was 20,000 m ³ / h, the supply air temperature was 140 ° C. The exhaust air temperature was set to 65 ° C by water evaporation of the solution. After 1 h the fluidized bed operated in batch was so full that the granulation was ended. The solidification was carried out with the 20% polymer solution used in Example 1 at a supply air of 110 ° C. The polymer content in the finished granulate was 7% by weight. The granules obtained were sieved between 0.8 and 1.6 mm. The bulk weight was 710 g / l.

Example 4

The granules obtained according to Example 2 were again in the fluidized bed apparatus introduced and there at 130 ° C supply air temperature and 65 ° C exhaust air with the previously used 20% polymer solution sprayed from the side, so that a 20 wt .-% Wrapping was created. Likewise, the granules obtained in Example 3 were again in the Fluid bed equipment introduced and there at 130 ° C supply air temperature and 65 ° C exhaust air sprayed with the 20% polymer solution from the side, so that a 10 wt .-% Wrapping was created.

Example 5

In a fluidized bed apparatus with a diameter of 15 cm (Glatt® AGT 1800), granules containing trimethylammonium acetonitrile methosulfate were sprayed with the polymer solution used in Example 1 using two-component nozzles arranged below. The supply air volume was 100 m ³ / h, the supply air temperature was 120 ° C and the exhaust air temperature 60 ° C. The two-component nozzles were operated with warm air at 75 ° C; the air factor of the nozzles was 1.5 (kg air / kg solution). The proportion of the coating layer in the finished granulate was 10% by weight. A complete coating layer was visible under the microscope. The granules obtained consisted of particles with diameters in the range from 0.8 mm to 2.0 mm and had a bulk density of 750 g / l.

Claims (12)

1. A process for the preparation of a coated particulate preparation comprising a compound of the formula (I),


in which R ^{1 is} -H, -CH ₃ , a C _2-24 alkyl or alkenyl radical, a substituted C _2-24 alkyl or alkenyl radical with at least one substituent from the group -Cl, -Br, - OH, -NH ₂ , -CN, an alkyl or alkenylaryl radical with a C _1-24 alkyl group, or for a substituted alkyl or alkenylaryl radical with a C _1-24 alkyl group and at least one further substituent on the aromatic ring, R ² and R ^{3 are} independently selected from -CH ₂ -CN, -CH ₃ , -CH ₂ -CH ₃ , -CH ₂ -CH ₂ - CH ₃ , -CH (CH ₃ ) -CH ₃ , -CH ₂ - OH, -CH ₂ -CH ₂ -OH, -CH (OH) -CH ₃ , -CH ₂ -CH ₂ -CH ₂ -OH, -CH ₂ -CH (OH) -CH ₃ , -CH (OH) - CH ₂ -CH ₃ , - (CH ₂ CH ₂ -O) _n H with n = 1, 2, 3, 4, 5 or 6, R ⁴ and R ⁵ independently of one another for R ¹ , R ² or R ³ have the meaning given and X is a charge-balancing anion, characterized in that the bleach activator of the formula (I), which is present in solid, in particular powdery form, is obtained sprayed in a mixture with binder and / or solid filler or as prefabricated granules, with simultaneous drying in a fluidized bed apparatus, with an acidic aqueous solution which contains polymeric polycarboxylate and / or phosphonic acid or alkali metal phosphonate as the coating and consolidation active ingredient. 2. The method according to claim 1, characterized in that the pH of the aqueous solution by adding sulfuric acid and / or citric acid to acid Sets values. 3. The method according to claim 1 or 2, characterized in that the aqueous solution has a pH in the range from 4 to 4.4. 4. The method according to any one of claims 1 to 3, characterized in that - based on the granules to be coated - sprayed as much of the aqueous solution that the Coating 1% by weight to 25% by weight, in particular 2% by weight to 15% by weight accounts. 5. The method according to any one of claims 1 to 4, characterized in that as Coating and solidifying agent a polymerization product of acrylic acid, Methacrylic acid or maleic acid or a copolymer of at least two of uses this and / or phosphonic acid or alkali phosphonate. 6. The method according to any one of claims 1 to 5, characterized in that a compound according to formula 1, in which R ¹ , R ² and R ^{3 are the} same and in particular mean methyl groups, is used. 7. The method according to any one of claims 1 to 6, characterized in that a compound of formula I is used in which the anion X ^- halide such as chloride, fluoride, iodide and bromide, nitrate, hydroxide, phosphate, hydrogen phosphate, dihydrogen phosphate, pyrophosphate , Metaphosphate, hexafluorophosphate, carbonate, hydrogen carbonate, sulfate, hydrogen sulfate, C _1-20 alkyl sulfate, C _1-20 alkyl sulfonate, optionally C _1-18 alkyl-substituted aryl sulfonate, chlorate, perchlorate and / or an anion of C _1-24 - Carboxylic acid such as formate, acetate, laurate, benzoate or citrate, alone or in any mixtures. 8. The method according to claim 7, characterized in that one uses a compound according to formula I, in which the anion X ^- chloride, sulfate, hydrogen sulfate, methosulfate, ethosulfate, C _12/18 -, C _12/16 - or C _13/15 Alkyl sulfate, lauryl sulfate, dodecylbenzenesulfonate, toluenesulfonate, cumene sulfonate, xylene sulfonate or mixtures thereof. 9. The method according to any one of claims 1 to 8, characterized in that the coated particulate preparation with an average particle diameter in the range from 0.2 mm to 2.5 mm, in particular in the range from 0.4 mm to 2.0 mm. 10. The method according to any one of claims 1 to 9, characterized in that the Bulk density of the coated particulate preparation in the range from 300 g / l to 1000 g / l, in particular in the range from 400 g / l to 800 g / l. 11. The method according to any one of claims 1 to 10, characterized in that the proportion of compound of formula (I) in the coated particulate preparation in Range from 10% by weight to 90% by weight, in particular from 15% by weight to 50% by weight lies. 12. Use of the coated particulate preparation available after Method according to one of claims 1 to 11, for the production of particulate Detergents or cleaning agents.